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中国精品科技期刊2020
戴尽波,沈洁,董文静,等. 微量QuEChERS-超高效液相色谱-串联质谱法检测凉茶中59种非法添加化学药物[J]. 新宝登录入口(中国)有限公司,2024,45(6):1−12. doi: 10.13386/j.issn1002-0306.2023040213.
引用本文: 戴尽波,沈洁,董文静,等. 微量QuEChERS-超高效液相色谱-串联质谱法检测凉茶中59种非法添加化学药物[J]. 新宝登录入口(中国)有限公司,2024,45(6):1−12. doi: 10.13386/j.issn1002-0306.2023040213.
DAI Jinbo, SHEN Jie, DONG Wenjing, et al. Determining the 59 Chemical Drugs Illegally Added in Herbal Tea by a Micro-QuEChERS-Based UPLC-MS/MS[J]. Science and Technology of Food Industry, 2024, 45(6): 1−12. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023040213.
Citation: DAI Jinbo, SHEN Jie, DONG Wenjing, et al. Determining the 59 Chemical Drugs Illegally Added in Herbal Tea by a Micro-QuEChERS-Based UPLC-MS/MS[J]. Science and Technology of Food Industry, 2024, 45(6): 1−12. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023040213.

微量QuEChERS-超高效液相色谱-串联质谱法检测凉茶中59种非法添加化学药物

Determining the 59 Chemical Drugs Illegally Added in Herbal Tea by a Micro-QuEChERS-Based UPLC-MS/MS

  • 摘要: 目的:建立一种微量QuEChERS(micro-QuEChERS)结合超高效液相色谱-串联质谱(UPLC-MS /MS)同时检测凉茶中59种非法添加药物的分析方法。方法:样品用乙腈超声提取5 min,提取液用NaCl及无水Na2SO4进行盐析分层,上清液用C18吸附剂进行净化后,经ACQUITY HSS T3(100 mm×2.1 mm,1.8 μm)色谱柱分离,以0.01%甲酸水溶液(A)-乙腈:甲醇(8:2)(B)为流动相进行梯度洗脱,并采用电喷雾正负离子多反应监测模式检测,空白基质外标法定量。结果:59种化合物在其线性浓度范围内,线性关系良好,决定系数均大于0.999,检出限为5.0~10.0 μg/L,定量限为10.0~25.0 μg/L。在25.0、50.0、100.0 μg/L 3个添加水平下,平均回收率为60.3%~128.8%(n=6),相对标准偏差(RSD)1.0%~13.7%。结论:该方法操作简单,净化效果好,灵敏度高,可用于凉茶中59种非法添加化学药物的快速分析。

     

    Abstract: Objective: An analysis method for simultaneous determination of 59 kinds of chemical drugs illegally added in herbal tea by micro-QuEChERS method combined with ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) was established. Method: The samples were extracted by ultrasonic extraction from acetonitrile solution for 5min and salted out with sodium chloride (NaCl) and anhydrous sodium sulfate (Na2SO4). Supernatant was purified with C18 sorbent and separated on a ACQUITY HSS T3 column (100 mm×2.1mm, 1.8 μm) by gradient elution using a mixture of 0.01% formic acid and acetonitrile: Methanol (8:2) as the mobile phase. Then the analytes were quantified by UHPLC-MS/MS in multiple reaction monitoring mode (MRM) via positive and negative electrospray ionization quantified by external standard method. Result: The coefficient of determination of the standard calibration curves for the 59 analytes were all above 0.9990. The limit of detection (LOD, S/N≥3) and the limit of quantitation (LOQ, S/N≥10) were 5.0~10.0 and 10.0~25 μg/L. At three spiked of 25.0, 50.0 and 100.0 μg/L, the average recoveries of 59 analytes were 60.3%-128.8% (n=6) with the relative standard deviations in the range of 1.0%~13.7%. Conclusion: The method developed was simple, sensitive, and had good purification effect. It could be applied for the rapid determination of 59 chemical drugs illegally added in herbal tea.

     

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